CN111883690A - Transparent metal electrode and preparation method thereof - Google Patents
Transparent metal electrode and preparation method thereof Download PDFInfo
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- CN111883690A CN111883690A CN201910802582.8A CN201910802582A CN111883690A CN 111883690 A CN111883690 A CN 111883690A CN 201910802582 A CN201910802582 A CN 201910802582A CN 111883690 A CN111883690 A CN 111883690A
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Abstract
The invention relates to a transparent metal electrode and a preparation method thereof. The method comprises the following steps: depositing ink on a substrate to form a liquid layer, wherein the ink comprises a solvent and metal nanoparticles; placing a mask plate above the liquid layer, controlling the solvent to volatilize, and obtaining a metal nano-particle accumulation body after the solvent is completely volatilized; and sintering the metal nano particle accumulation body to obtain the transparent metal electrode. The method can realize the preparation of the high-precision metal grid electrode without material waste under a simple process.
Description
Technical Field
The invention relates to the technical field of light-emitting devices, in particular to a transparent metal electrode and a preparation method thereof.
Background
The structure of an electroluminescent device generally comprises: an anode, a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer, and a cathode. When the anode or the cathode is on the light-emitting side, transparent electrodes are needed to be selected, because the transmittance of the transparent electrodes directly affects the light-emitting efficiency of the electroluminescent device. In addition, the transparent electrode needs to have better conductivity, which directly leads to the increase of the starting voltage of the electroluminescent device.
Common transparent electrodes include ITO (indium tin oxide) and metallic silver thin films of 5-25nm, etc. However, although ITO has a good transmittance, it has a large resistance, requires a high temperature process, and has poor flexibility, and thus it cannot adapt to the development trend of future flexible displays. Although the metal silver film has good conductivity and transmittance, the metal silver itself has reflection, so that a microcavity is easily formed in the electroluminescent device, and the viewing angle characteristic of the electroluminescent device is further influenced. Therefore, a metal mesh electrode capable of taking into account conductivity, transmittance and low reflection characteristics is one of the development directions of future transparent metal electrodes, and fig. 1 shows a bottom-emitting OLED device using a metal silver mesh electrode as an anode.
The current methods for preparing the metal grid electrode mainly comprise photoetching and printing. The photoetching precision is higher, smaller line width can be realized, but the manufacturing process is complicated, the cost is higher and the material utilization rate is low; although the printing process is simple and no material is wasted, the printing precision is low, and the line width of more than 50um can be realized.
Disclosure of Invention
Based on the above, the invention provides a preparation method of a transparent metal electrode, which can realize the preparation of a high-precision metal grid electrode without material waste under a simple process.
The specific technical scheme is as follows:
a preparation method of a transparent metal electrode comprises the following steps:
depositing ink on a substrate to form a liquid layer, wherein the ink comprises a solvent and metal nanoparticles;
placing a mask plate above the liquid layer, controlling the solvent to volatilize, and obtaining a metal nano-particle accumulation body after the solvent is completely volatilized;
and removing the mask plate, and sintering the metal nano particle accumulation body to obtain the transparent metal electrode.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method of the transparent metal electrode, the difference of solvent volatilization rates is made by using a mask plate, so that a surface tension gradient is formed to drive the solvent-wrapped metal nanoparticles to flow directionally, and thus the metal nanoparticles of continuous net-shaped patterns are accumulated, the metal nanoparticles are sintered to obtain the metal grid electrode, namely the transparent technical electrode, and the preparation of the high-precision metal grid electrode without material waste is realized under a simple process. The mechanism is as follows:
the mask plate is provided with an opening area and a covering area, when the mask plate is placed above a liquid layer formed by ink, the liquid layer corresponding to the opening area of the mask plate is a normal volatilization area, and the liquid layer corresponding to the covering area of the mask plate is a volatilization inhibition area. In a standing state, the solvent of the liquid layer naturally volatilizes, the solvent volatilization speed of the 'normal volatilization zone' is higher than that of the 'volatilization inhibition zone', and the volatilization of the solvent can take away a part of heat, so that the temperature of the surface of the liquid layer of the 'normal volatilization zone' is lower than that of the surface of the liquid layer of the 'volatilization inhibition zone', and the liquid on the surface of the liquid layer is driven to flow from the 'volatilization inhibition zone' to the 'normal volatilization zone' by the surface tension gradient generated by the temperature gradient. Meanwhile, in order to replenish the liquid on the surface of the liquid layer of the "volatilization suppression zone", a flow of the liquid from the "normal volatilization zone" to the "volatilization suppression zone" is formed at the bottom of the liquid layer, and a marangoni reflux as shown in fig. 2 is formed. The marangoni reflow carries the metal nanoparticles in the liquid layer (i.e., the ink), and after the solvent in the liquid layer is completely volatilized, the metal nanoparticles can be stacked on the substrate corresponding to the masking area. The metal nano particles are stacked and sintered at high temperature, so that a relatively compact metal structure, namely a metal grid electrode can be obtained.
In the prior art, if the metal grid electrode is directly printed by ink jet printing, the line width of the grid is limited by the size of ink drops. At present, an industrial-grade printer generally generates about 5pL of ink drops, the diameter of the ink drops is about 21.2um, and considering that the ink drops are further spread on a substrate (the diameter after spreading is about 40-50 um), the line width of the ink drops can only be more than 50 um. By adopting the preparation method, the line width is only limited by the processing precision of the mask, the line width of several microns can be easily realized, and the fineness is close to that of the metal grid electrode obtained by direct photoetching.
Drawings
FIG. 1 is a diagram of a bottom-emitting OLED device structure;
FIG. 2 is a schematic of Marangoni reflow formation;
FIG. 3 is a schematic diagram of relative positions of a substrate, a liquid layer and a mask;
FIG. 4 is a first schematic diagram of a mask structure;
FIG. 5 is a schematic diagram of a metal nanoparticle stack with a mesh pattern;
FIG. 6 is a schematic diagram of a metal nanoparticle stack with a mesh pattern;
FIG. 7 is a schematic view of heating a metal nanoparticle stack;
FIG. 8 is a second schematic diagram of a mask structure;
FIG. 9 is a third schematic view of a metal nanoparticle stack with a mesh pattern;
FIG. 10 is a third schematic view of a mask structure;
fig. 11 is a fourth schematic view of a metal nanoparticle bank with a mesh pattern.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
A preparation method of a transparent electrode comprises the following steps:
the metal nanoparticles can be silver, copper, aluminum and other metals with good conductivity, i.e., the metal nanoparticles can be one or more selected from silver nanoparticles, copper nanoparticles and aluminum nanoparticles. But silver nanoparticles are most preferable in view of stability of the metal nanoparticles in an atmospheric environment.
It is understood that the size of the metal nanoparticles is between 200nm and 500 nm.
When the ink is prepared, the metal nano particles are added into the solvent, wherein the volume fraction of the metal nano particles in the ink is between 0.1 and 2 percent. The solvent used may be a low boiling point solvent such as ethanol, cyclohexane, toluene, xylene, anisole, etc.
It is understood that the method of depositing the ink includes, but is not limited to, spin coating or ink jet printing, and the ink is deposited on the entire surface of the substrate. After depositing the ink, a liquid layer is obtained due to the effect of the surface tension of the liquid. The thickness of this layer is preferably 50 μm to 300. mu.m.
And 2, placing a mask plate above the liquid layer, controlling the solvent to volatilize, and obtaining the metal nano-particle accumulation body after the solvent is completely volatilized.
Specifically, a mask plate is obtained, the mask plate is provided with a plurality of opening areas distributed in an array mode, the rest of the opening areas are covering areas, the mask plate is placed above the liquid layer, the volatilization rate of a solvent in the liquid layer corresponding to the opening areas is larger than that of the solvent in the liquid layer corresponding to the covering areas, and after the solvent in the liquid layer is completely volatilized, the metal nano particle accumulation body is obtained on a substrate corresponding to the covering areas.
Under the normal temperature state of stewing, the solvent natural volatilization of liquid layer, the speed of volatilizing of mask plate meeting hindrance corresponding position department liquid layer solvent. Namely, the liquid layer solvent volatilization rate of the normal volatilization zone corresponding to the opening area of the mask plate is faster than that of the volatilization inhibition zone corresponding to the mask plate covering area. Preferably, the mask is spaced from the liquid layer by 10 μm to 200 μm to facilitate formation of a marangoni reflow. More preferably, the distance between the liquid layer and the mask plate is 10-50 μm, and the closer the liquid layer and the mask plate are, the more favorable the Marangoni reflow is.
Because the solvent volatilization speed of the normal volatilization zone is faster than that of the volatilization inhibition zone, and the volatilization of the solvent can take away a part of heat, the temperature of the surface of the liquid layer of the normal volatilization zone is lower than that of the surface of the liquid layer of the volatilization inhibition zone, and the surface tension gradient generated by the temperature gradient drives the liquid on the surface of the liquid layer to flow from the volatilization inhibition zone to the normal volatilization zone. Meanwhile, in order to replenish the liquid on the surface of the liquid layer of the "volatilization suppression zone", a flow of the liquid from the "normal volatilization zone" to the "volatilization suppression zone" is formed at the bottom of the liquid layer, and a marangoni reflux as shown in fig. 2 is formed. The marangoni reflow carries metal nanoparticles in a liquid layer (i.e., ink), and the metal nanoparticles are carried by the lower portion of the marangoni reflow, deposited in a specific region corresponding to a masking region of a mask, and form a pile. After the solvent of the liquid layer is completely volatilized, metal nano-particle stacks can be formed at the positions of the substrate corresponding to the masking areas.
In fact, the area of the substrate where volatilization is inhibited is slightly smaller than the area covered by the mask plate, so the line width of the finally formed metal grid is slightly smaller than the width of the mask plate.
Further, the shape of the opening region of the mask plate may be any shape, preferably a polygon or a circle. Wherein the polygon may be a rectangle. More preferably, the shape of the opening region is circular. Because the volatilization rates of all positions on the edge of the circular opening of the mask plate are equal, the carrying effect of the Marangoni reflow is the same, the formed pattern of the metal nano particles accumulated is also circular, and the line width of the grid is easy to control. When the polygonal opening is adopted, the volatilization rate at the corner is obviously smaller than the side length position, the difference of the volatilization rates of the two is changed along with the drying condition and the ink change, and the finally formed accumulated pattern is difficult to control, so that the line width of the grid is difficult to accurately adjust, and the process difficulty is increased.
When the open regions of the mask are circular, the diameter D1 of the preferred circle is 150 μm-250 μm, and the distance D2 between the centers of two adjacent open regions in the same row is 300 μm-1000 μm.
And 3, sintering the metal nano particle accumulation body to obtain the transparent metal electrode.
It can be understood that the mask plate is removed, and then the metal nano particles are piled up and heated at 120-200 ℃ for 10-30 min, so that the metal nano particles are sintered into a relatively compact metal structure, namely the transparent metal grid electrode.
In the prior art, if the metal grid electrode is directly printed by ink jet printing, the line width of the grid is limited by the size of ink drops. At present, an industrial-grade printer generally generates about 5pL of ink drops, the diameter of the ink drops is about 21.2um, and considering that the ink drops are further spread on a substrate (the diameter after spreading is about 40-50 um), the line width of the ink drops can only be more than 50 um. By adopting the preparation method, the line width of the metal grid is not limited, the line width is only limited by the processing precision of the mask, the line width of several micrometers can be easily realized, the fineness is close to that of the metal grid electrode obtained by direct photoetching, and the processing precision is high. Meanwhile, the prepared transparent metal electrode has the advantages of simple process, no need of expensive photoetching equipment, low production cost, short processing time and high production efficiency, and compared with the traditional printing process, the transparent metal electrode has no material waste. In addition, the invention can design the position and the shape of the opening area and the masking area of the masking plate according to the required metal network.
Example 1
The embodiment provides a preparation method of a transparent metal electrode, which comprises the following steps:
and S1, adding the metal silver nanoparticles into the solvent to obtain the ink.
And S2, depositing the ink on the whole area of the substrate by adopting an ink-jet printing method to form a liquid layer H1, wherein the thickness of the liquid layer H1 is about 100 mu m.
S3, placing a mask above the liquid layer, as shown in fig. 3, wherein 1 is a substrate, 3 is a liquid layer, and 2 is a mask, standing at normal temperature to allow the solvent in the liquid layer to volatilize naturally in the atmosphere, thereby forming marangoni reflux, as shown in fig. 2. Wherein the distance H2 between the liquid layer and the mask plate is 100 μm, said mask plate being provided with open areas and masked areas, as shown in fig. 4. The opening regions are distributed in an array shape, the shape is circular, the diameter D1 of the circle is 200 mu m, and the distance D2 between the centers of two adjacent opening regions in the same row is 600 mu m. The rate of evaporation of the solvent from the liquid layer corresponding to the open areas is greater than the rate of evaporation of the solvent from the liquid layer corresponding to the masked areas.
S4, after the solvent in the liquid layer is completely volatilized, as shown in fig. 5 and 6, a continuous net-shaped pattern metal nanoparticle stack 31 is formed on the substrate corresponding to the masked region.
Since the area of the substrate with suppressed volatilization is slightly smaller than the area covered by the mask plate, the line width of the finally formed metal grid is slightly smaller than the width of the mask plate. The hatched portion is clearly thinner in fig. 6 than in fig. 4.
S5, removing the mask plate, and heating the metal nanoparticles at 160 ℃ for 20min to sinter the metal nanoparticles into a relatively dense metal structure 32, i.e., a transparent metal mesh electrode, as shown in fig. 7.
Example 2
The embodiment provides a preparation method of a transparent metal electrode, which comprises the following steps:
and S1, adding the metal silver nanoparticles into the solvent to obtain the ink.
And S2, depositing the ink on the whole area of the substrate by adopting an ink-jet printing method to form a liquid layer H1, wherein the thickness of the liquid layer H1 is about 100 mu m.
S3, placing a mask plate above the liquid layer, keeping a distance H2 between the liquid layer and the mask plate at 100 mu m, standing at normal temperature, and naturally volatilizing the solvent of the liquid layer in an atmospheric environment to form Marangoni reflux. The mask plate is provided with an opening region and a masking region, as shown in fig. 8. The opening regions are distributed in an array shape, the shape is circular, the diameter D1 of the circle is 200 mu m, and the distance D2 between the centers of two adjacent opening regions in the same row is 600 mu m. The rate of evaporation of the solvent from the liquid layer corresponding to the open areas is greater than the rate of evaporation of the solvent from the liquid layer corresponding to the masked areas.
S4, after the solvent in the liquid layer is completely volatilized, forming a continuous net-shaped pattern metal nanoparticle accumulation body on the substrate corresponding to the covering area, as shown in FIG. 9;
since the area of the substrate with suppressed volatilization is slightly smaller than the area covered by the mask plate, the line width of the finally formed metal grid is slightly smaller than the width of the mask plate. The hatched portion is significantly thinner in fig. 9 than in fig. 8.
S5, removing the mask plate, and heating the metal nano-particle stack at 160 ℃ for 20min to sinter the metal nano-particle stack into a relatively compact metal structure, namely a transparent metal grid electrode.
Example 3
The embodiment provides a preparation method of a transparent metal electrode, which comprises the following steps:
and S1, adding the metal silver nanoparticles into the solvent to obtain the ink.
And S2, depositing the ink on the whole area of the substrate by adopting an ink-jet printing method to form a liquid layer H1, wherein the thickness of the liquid layer H1 is about 100 mu m.
S3, placing a mask plate above the liquid layer, keeping a distance H2 between the liquid layer and the mask plate at 100 mu m, standing at normal temperature, and naturally volatilizing the solvent of the liquid layer in an atmospheric environment to form Marangoni reflux. The mask plate is provided with an opening region and a masking region, as shown in fig. 10. The opening areas are distributed in an array and are rectangular in shape. The rate of evaporation of the solvent from the liquid layer corresponding to the open areas is greater than the rate of evaporation of the solvent from the liquid layer corresponding to the masked areas.
S4, after the solvent in the liquid layer is completely volatilized, forming a continuous net-shaped pattern metal nanoparticle accumulation body on the substrate corresponding to the covering area, as shown in FIG. 11;
since the area of the substrate with suppressed volatilization is slightly smaller than the area covered by the mask plate, the line width of the finally formed metal grid is slightly smaller than the width of the mask plate. The hatched portion is significantly thinner in fig. 11 than in fig. 9.
S5, removing the mask plate, and heating the metal nano-particle stack at 160 ℃ for 20min to sinter the metal nano-particle stack into a relatively compact metal structure, namely a transparent metal grid electrode.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (11)
1. A preparation method of a transparent metal electrode is characterized by comprising the following steps:
depositing ink on a substrate to form a liquid layer, wherein the ink comprises a solvent and metal nanoparticles;
placing a mask plate above the liquid layer, controlling the solvent to volatilize, and obtaining a metal nano-particle accumulation body after the solvent is completely volatilized;
and sintering the metal nano particle accumulation body to obtain the transparent metal electrode.
2. A production method according to claim 1, wherein a space between the liquid layer and the mask plate is 10 μm to 200 μm.
3. A production method according to claim 1, wherein a space between the liquid layer and the mask is 10 μm to 50 μm.
4. The manufacturing method according to claim 1, wherein the mask plate is provided with a plurality of opening regions distributed in an array.
5. The method of claim 4, wherein a shape of a plurality of the open regions is circular.
6. The method of claim 5, wherein the diameter of the circle is 150 μm to 250 μm.
7. The method of claim 4, wherein a shape of a plurality of the open regions is a polygon.
8. A method of manufacturing as claimed in any of claims 1-7, characterized in that the thickness of the liquid layer is 50 μm-300 μm.
9. The method for preparing a silver nanoparticle, a copper nanoparticle and an aluminum nanoparticle, according to any one of claims 1 to 7, wherein the metal nanoparticles are selected from one or more of silver nanoparticles, copper nanoparticles and aluminum nanoparticles.
10. The method according to any one of claims 1 to 7, wherein the solvent is one or more selected from the group consisting of ethanol, cyclohexane, toluene, xylene, and anisole.
11. A transparent metal electrode produced by the production method according to any one of claims 1 to 10.
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| CN113991032A (en) * | 2021-10-28 | 2022-01-28 | 湖南恒显坤光电科技有限公司 | Novel transparent OLED device |
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| US20120080218A1 (en) * | 2010-09-30 | 2012-04-05 | Da-Ren Chiou | Transparent conductive film having high optical transmittance and method for manufacturing the same |
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